Apparatus for producing ether.



D. ANNARATONE.

' APPARATUS FOR PRODUCING ETHER.

APPLICATION FILED NOV.22,1909. 1,067,709. Patented July 15, 1913.

2 SHEETS-SHEET 1.

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APPARATUS FOR PRODUCING ETHER;

APPLIOATZGK FILED NOV. 22, 1909.

Patented July 15, 1913.

2 SHEETS-*SHEET 2.

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WITNESSES DUILIO ANNARATONE, OF SETTIMO TOBINESE, NEAR TUBIN, ITALY.

APPARATUS FOR PRODUCING ETHER.

Specification of Letters Patent.

Patented July 15, 1913.

Application filed November 22, 1809. Serial No. 529,223.

To all whom it may concern:

Be it known that I, DUILIO ANNABAIONE, a subject of the King of Italy, and a resident of Settinio T orinese, near Turin, Italy, have invented certain new and useful Improvements in Apparatus for Producing Ether, of which the following is a fu'lh'clea-r, and exact description.

The present invention relates to an apparatus for producing ether, my purpose being to render the apparatus highly productive and at the some timecomparatively cheap in operation, especially as regards the quell tity of fuel and manual labor required.

My invention has, moreover, the advantages of simplicity and compactness.

In the drawings, Figure 1 is a diagrammatic view of the apparatus, Fig. 2 is a centrill vertical serion of the ethcrilier and su perheater, and Fig. 3 is a vertical sect-ion of the cooling tank.

A reservoir S, sunken below the surface of the earth, is used as a reservoir for bold ing the alcohol to he etheriytied. Jonnected withthis reservoir is e pump P, the stroke of which is variable at will for controlling the alcohol to be used from the reservoir.

At M is a superheater formed of a steam tight reservoir containing a heating coil adapted to be heated by steam under pressure.

At- E is an etherilier having t N form. of an iron reservoir lined intcrnollifr with lead or with some other material capable of resisting the action of sulfuric acid. This reservoir is filled to a predetermined height with small pieces of sandstone for the purpose of sulju'lividing the vspor into innumerable small streams and toprevont the too rapid mixture of the etherifying fluid therewith during the process of etheriticution.

The bottom of the reservoir E is heated by any appropriate means, such, for instance, as a heating pipe made of lead and supplied with steam under pressure.

Connected with the reservoir E is a pipe 4 which leads downwardly from a vat 7 2 containing sulfuric acid. A siphon pipe 3 is connected with the reservhir E and is used for discharging an excess of acid from the reservoir E. That is to say, the acid in this reservoir can never clinih higher then By arrangement the top of the siphon pipe. of the pipes inside of the IQSelltill E, the liquid that floivs out of this reservoir is drawn from the lowermost part thereof,

While the liquid entering this reservoir is admitted at the top and has more on. less tendency to remain there. The siphon pipe 3 is connected with the reservoir E and serves for discharging the excess of acid from the reservoir E into the reservoir A thermometer in and a manometer as disposed at the top of the reservoir E indicate the internal pressure and temperature of this reservoir. A cleaning apparatus A. is provided for removing impurities from the other. This cleaning apparatus is formed of two or three segments, each of which sup ports a. plate of the kind usually employed in other cleaning. apparatus. At X X is a vet containing a solution of sods. and con nected with this vat is a pipe 2 which leads down to the cleaning apparatus A. The sc lution of soda entering this cleaning apparatus descends gradually from one plate to the other, thereby filling the several segments up to a certain level. Connected with the last segment is a siphon pipe 7 through which the solution of soda is discharged from the cleaning apparatus.

The vapor to be cleaned through the cleaning apparatus A in a direction con trary to the'direction of travel of the solution, of soda, the vapor thus hubhlin up through the solution on the various p ates.

,A tower or column B, of the usual type employed for rectifying alcohol, is provided in connection with this apparatus and is supplied with water circulation by means of an attachment B provided for the urpose. A. somewhat similar tower Q o: the type usually employed for rectifying ether is provided with an attachment C for supplying water circulation. to the tower C and also with a. reservoir at the hot-torn C" which is heated by a heating coil. A cooling tank F is provided with two heating coils, one being formed of a pipe of large diameter and making turns of considerable width and having its inlet at O and its outlet at T. A second heatin coil is mounted inside of the first one an is formed by a very long pipe of smaller diameter, having an inlet at U and an outlet at T; The tower or column H with its contents-is heated from the bottom directly by a steam jet.

ion

The pipe 8 puts in communication the hausting column H with the column B. The pipes 3--9 --7-l1 serve. as discharging siphons respectively for the apparatus and brought up from the reservoir 8 by means of the pipes 12 or 13. The other am gases, by coming out of the column or tower (l, are brought through the pipe 14 to the coil contained in the tank F, Where the other is condensed, thence goes out through the spherical reservoir T, and filling the pipes V, V, V" up tothe height indicated by the letter I collects in the reservoir (.2 from which it is extracted by aid of the valve R, and may then be utilized.

The gases fell-owing the other up to the valve T, being unable to pass through the tube V because the latter is filled with lie uid, go through the pipe 18 and are com-- polled to run through the heating coil oil the reservoir F which is very long and has a short diameter. In this reservoir the vapor of the ether escaping from the coil is condensed, the ether goes out through the spherical reservoir '1 and thence .thrmigh the tubes V and V to the reservoir Q while the gases, divested of every trace of ether,

0 through the pipe 19 and are discharged Into the atl'nosphcre. Test tubes X, Y, Z are provided in connection with the coil or con denser G. The tube X indicates the degree of-alcohol returning into the reservoir. The tube Y indicates whether or not the Waters coming from the column H are completely exhausted, and the tube Z indicates the de gree of ether produced. The action of the apparatus is controlled largely 3y means of the valves 20. 21, 22, '23, the valves 20 and 23 controlling respectively the supply of water to the towers B and C. The valve ill controls the supply of vapor in the exhaust column of the Water. The valve 22 controls the vapor in the coil of the tank C". The heating of this tank has the object ot'elinnii nat-ing a small quantity of other which may be contained in the alcohol to be returned to the reservoir S. o

By means of the arrangement adopted in my apparatus, the inconvenience of all other apparatus of other'systcms constructed up to date, is avoided; of requiring to prepare separately the mixture of sulfuric acid and of ethylic alcohol to be introduced into the etherifier. The continuous introduction of sulfuric acid maintains in the mixture a constant etherifying power. Since the mixture cannot be exhausted it never changes, and the apparatus may Work for a good many months consecutively without stopping.

The superheater (which may he as rle scribed, and also substituted by any other suitable means for evaporating and superheating the alcohol) is intended to prevent the passing of the heat between the acid of the etherifier and the alcohol to be cthcrifierl. In other apparatus of other systems in which the alcohol is introduced into the etherifier liquid and cold there is a formation of a. large quantity of secondary products (on account. of the prolonged Contact of the alcohol with the acid) which reduces the production of other. In appl-icants case, contrariwise, the etherifica-tion is very rapid, the alcohol remains in contact with the acid a very short time, consequently the tonnation of secondary products is considerably reduced. j

By using the alcohol in the: fox-mot superheated vapor, thereis the advantage of being able to reduce. the masses of etlzertfiaut liquid without reducing the production of the apparatus; consequently very smalt ethe-rifiers can be used with "a great eclmomy of the installation and the consumption heat to super-heat them.

It is not nccessa-ry to mix the sulfuric afiid and the ethyl alcohol prior to admission to the apparatus, since this mixture t-a'kes place in the 'supe'rheatier M, and any other suitable means may be employed for mixing the acid and the alcohol if desired.

The etherificatio'n is veryreadily obtained by aid of this apparatus, although hereto fore it has in other apparatus been very slow.

()wing to the rapidity of the process as carried out by the foregoing apparatus, the formation of the secondary products is reduced considerably.

employing superheated alcohol there results the advantage of reducing the masses of etherifyin'g liquid without reducing the amount of the product.

Moreover, an apparatus of the kind above described may be made very small. and compact. for a given output, thereby attaining considerable economy both in the installation and in the fuel required for heating.

Aside from the foregoing advantages, the work of the apparatus is comparatively constanls and continuous, it not being necessary to stop the work of the apparatus for any reason.

By using the cooling apparatus F with its double coil, the gases first pass into the lower portion of the "apparatus and then through the coolest portion of the Water, so that the gases come out entirely eX- haustcd. 3

The pump takes the alcohol out of the reservoir exactly in the quantity required for its conversion into ether, and pumps it into the superheater WVllGIG itis evaporated and heated to a temperature of 130 degrees C. From here the vapors are fed from below through a pipe into the receptacle, lined with lead or other material not attacked by sulfuric acid and filled up to a determined height with stone halls in order to properly divide the vapors. Here the vapor comes in contact with the sulfuric acid and is converted into raw ether. The raw ether produced in this manner, goes in the vaporous through. After a certain time the level of and during the further state, through the liquid quickly and arrives" lathe receptacle, where the drops of sul-' fi ric acid carried along mechanically. are left behind and then passes through a pipe into the cleaning device. At the beginning i of thereaction' the sulfuric acid contained 5 in the receptacle is heated to 130 degrees-C., l operation no further heating is required. The sulfuric acid becomes exhausted after some time, and this defect is remedied by letting in continuously, drop by drop, fresh sulfuric acid. The siphon draws oif a corresponding quantity of exhausted acid. The cleaning device containing sodium hydroxid binds the sulfurous acid and the impurities, while ether, water and the gases pass through the liquid one after the other quicker or slower and are then cooled. The rectifying devices and the distilling device are arranged in such manner that only vapors at a temperature lower than .80 degrees C. can pass the liquid consisting of water, and sodium hydreeiid raises in t e last compartment of the'cleaner, so that the ether can pass into the exhauster column, where the last traces of alcohol are removed. In this column the liquid falls from compartment to compartment, While the current of vapor comes from below, moves from top to bottom and sweeps along the alcoholic vapors. These are returned into the column. The amount of the soda solution flowing downward in the cleaner is regulatedby means of a valve in such manner that the liquid on leaving through the siphon has a neutral reaction.

Having thus described my invention, I

claim as new and desire to secure by Letters- Patent:

1. A device of the character specified, comprising a reservoir for alcohol, a reaction vessel, a superheater, means for conducting alcohol to the superheater and for conducting the gasified alcohol to the reaction vessel and for delivering the said gasified alcoholto the vessel'at the bottom thcreof, means for conducting sulfuric acid to the reaction vessel and for introducing it near, the bottom thereof adjacent to the entering- 2. An apparatus for the uninterrupted production of ether out of ethyl alcohol. and sulfuric acid, comprising a device for superheating the alcohol, and a container partially filled withstone balls for holding the sulfuric acid and the superheated alc0 hol steam during the reaction between them, means for adding, continuously, alcohol and fresh sulfuric acid to the said container, pnd means in connection with the said'contamer for withdrawing a continuous stream of used acid therefrom. 7

In witness whereof, I have hereunto signed my name in the presence of two subscribing witnesses.

DUILIO ANNARATONE.

Witnes Pm zizh .GLiNOHO,

Fnntx sums. 

